Some aspects of the procedures to measure dissolved organic matter (DOM) released by phytoplankton account for important sources of errors. These aspects include: cell damage upon filtration of samples, residual inorganic 14C in the filtrates, NaH14CO3 ampoule contaminations and the low radiation activity proper to the released samples. Some experiments on these procedural problems were carried out and their effects on the released DOM were evaluated. A procedure to use control samples to avoid errors in the technique of DOM analysis by the liquid cintillation counter is described. Experiments on the validity of stocking preserved filtrates of natural plankton populations and algal cultures were also carried out for long periods prior to the radioactivity measurements.